An Improved Method for the Synthesis of [ZnW12O40](6-) and Its Reaction with [Pt(OH)(4)(H2O)(2)]: Crystal Structures of (H2NMe2)(5)H[ZnW12O40]center dot 3.5H(2)O and K6Na2[PtW6O24]center dot 11H(2)O

摘要

(Me2NH2)(5)H[ZnW12O40] center dot 3.5H(2)O (I) has been synthesized by the reaction between Zn(NO3)(2) center dot 4H(2)O, Na2WO4 center dot 2H(2)O and (Me2NH2)NO3 under hydrothermal conditions with a yield of 79%. The crystal structure of complex I has been characterized by single-crystal X-ray diffraction. Crystals of complex I are monoclinic, space group Cc, a = 13.165(1) angstrom , b = 19.370(1) angstrom, c = 20.987(2) angstrom , alpha = 84.81 degrees, V = 5145.9(0) angstrom(3), Z = 4, C10H48N5O43.5ZnW12. The Zn-O and W-O bond lengths are 1.86(2)-1.89(3) and 1.697(1)-2.030(2) , respectively. Na2K6[PtW6O24]center dot 11H(2)O (II) has been synthesized by a slow reaction between (Me2NH2)(5)H[ZnW12O40]center dot 3.5H(2)O and [Pt(OH)(4)(H2O)(2)] in H2O at room temperature. Crystals of complex II are trigonal, space group R (3) over barm, a = 13.138(1) angstrom, c = 20.987(2) angstrom, V = 2742.9(1) angstrom(3), Z = 3, H22O35Na2K6PtW6. The crystal structure of complex II contains [PtW6O24](6-) anions linked to K+ cations via oxygen atoms. The Na+ cation is coordinated to water molecules. The Pt atom is in a standard octahedral surrounding (Pt-O and W-O are 2.018(6) and 1.762(5)-2.151(4)angstrom, respectively).